研究生: |
黃昶閔 Chang-Min Huang |
---|---|
論文名稱: |
矽橡膠/環氧樹脂硬化反應與IPN結構之研究 A study on curing reaction & interpenetrating polymer networks structure of silicone rubber and epoxy resin blend |
指導教授: |
邱顯堂
Hsien-Tang Chiu |
口試委員: |
邱士軒
Shih-Hsuan Chiu 游進陽 Chin-Yang Yu 吳昌謀 Chang-Mou Wu 邱智瑋 Chih-Wei Chiu |
學位類別: |
碩士 Master |
系所名稱: |
工程學院 - 材料科學與工程系 Department of Materials Science and Engineering |
論文出版年: | 2013 |
畢業學年度: | 101 |
語文別: | 中文 |
論文頁數: | 88 |
中文關鍵詞: | 矽橡膠 、環氧樹脂 、高分子網目穿插 、相容性 |
外文關鍵詞: | silicone rubber, epoxy resin, IPN, miscibility |
相關次數: | 點閱:330 下載:6 |
分享至: |
查詢本校圖書館目錄 查詢臺灣博碩士論文知識加值系統 勘誤回報 |
本研究主要以高分子混摻(polymer blend)方式將矽橡膠(silicone rubber)與環氧樹脂(epoxy resin)做結合,先以流變儀(Rheometer)決定加工時間和熱示差掃描量熱儀(DSC)決定加熱溫度著手,再探討混合後的情況,以熱動態機械分析(DMA)探討其相容性,以拉伸試驗探討其應力應變,以熱重損失分析(TGA)探討其耐熱性的變化,以接觸角(Contact angle)探討其混合相之親水疏水效果,最後以電子顯微鏡(SEM)觀察其相分離狀況。本研究中為使兩相混合情況更趨一相,亦另添加改質劑矽烷耦合劑(Silane)和吡咯(Pyrrole),矽烷耦合劑在矽氧鍵部分能與矽橡膠反應,胺鏈端能對環氧基開環,而吡咯部分是雙鍵對矽橡膠之末端雙鍵作加成聚合,氮原子攻環氧基開環。在熱重損失部分,隨著矽橡膠比例增加,熱裂解溫度也隨之提高,代表熱穩定性有趨勢的延後,殘渣量的提高,代表熱安定性也跟著提高。在動態機械分析中,以SE55為相容性最佳,且Tg點提高超出原環氧樹脂,其熱性質也隨之提高,加入改質劑後也使兩相拉近,節點增加,代表其網目糾結程度增加。在拉伸試驗中,以SE82比例為佳,加入改質劑後,吡咯(Pyrrole)的效果提升更為明顯。在接觸角中,加入改質劑對疏水效果都有明顯的提升。
This study focuses on synthesis of silicone rubber/epoxy resin composites using polymer blend method. First of all, we used rheometer to determine processing time and dynamic scanning calorimetry (DSC) for optimum process temperature as well. Secondly to evaluate the composites, the dynamic mechanical analysis (DMA) was used for investigating miscibility, thermal gravimetric analysis for thermal resistance, tensile testing for stress-strength analysis, contact angle analysis for Hydrophobic and Hydrophilic effects, and scanning electronic microscopy (SEM) for observing phase separation. Moreover, to obtain the better miscibility and molecular entanglement, we added silane and pyrrole to modify the reaction. In silane part: Si-O can react with silicone rubber and amine result in ring-opening of epoxide group. In pyrrole part: addition polymerization with silicone rubber and nitrogen atom attribute ring-opening in epoxide group. As a result, the more silicone rubber added in composites, the better thermal resistance was obtained. In DMA testing, SE55 composite (Silicone/Epoxy: 5:5) shows the best miscibility and enhance in thermal properties due to the increase in Tg. In the tensile testing, SE82 (Silicone/Epoxy: 8:2) composite has best performance. And hydrophobic property improved for both modifiers added in the composites.
[1]M. Ebelmen, Ann. Chem, vol. 52-332, 1844.
[2]C. Friedel and A. Laddenburg, Ann. Chem, vol. 127-31, 1871.
[3]D. I. Mendeleev, Ed., The principles of Chemistry. London, 1891, p.^pp. Pages.
[4]W. Noll, Ed., Chemistry and Technology of siloxanes. New York: Acedemic Press, 1968, p.^pp. Pages.
[5]張招貴, 劉峰, and 余政, Eds., 有機矽化合物化學. 北京, 2010.3, p.^pp. Pages.
[6]C. Eaborn, Ed., Organosilicone compound. London: Butter Worths scientific plublication, 1962, p.^pp. Pages.
[7]P. R. Dvornic and R. W. Lenz, Eds., High Temperature Sioxane Elastomer. Basel,Heidelberg,New York, 1990, p.^pp. Pages.
[8]K. E. Plomanteer, Ed., Current Perspectives on Silicone Rubber Technology. Rubber Chemistry and Technology V, 1981, p.^pp. Pages.
[9]E. L. Warrick, Ed., Forty Year of First. McGraw-Hill Publishing Corp, 1990, p.^pp. Pages.
[10]W. Noll, Ed., Chemistry and Technology of siloxanes. New York: Acedemic Press, 1968, p.^pp. Pages.
[11] M. V. Beylen, M. Bolke, S. Bywater, E. Franta, P. Hallpap, J.-E. Hertz, et al., "Polym. Sci.," p. 1, 1988.
[12] 吳紹榮, "環氧樹脂/聚氧化二甲苯摻合體反應性,相行為及機械性質之研究," 博士, 化學工程研究所, 國立中央大學, 桃園縣, 2000.
[13] K. Matsukawa, K. Hasegawa, H. Inoue, A. Fukuda, and Y. Arita, "Preparation and curing behavior of siloxane‐containing epoxy resins," Journal of Polymer Science Part A: Polymer Chemistry, vol. 30, pp. 2045-2048, 1992.
[14] S. Lee and S. C. Kim, "Physical aging of polydimethylsiloxane‐modified epoxy resin," Journal of applied polymer science, vol. 69, pp. 1291-1300, 1998.
[15] 陳俊男, "溶膠-凝膠法製備環氧樹脂/聚矽氧烷之混成材料研究," 碩士, 化學學系碩士班, 淡江大學, 新北市, 2005.
[16] L. H. Sperling, Ed., Interpenetrating Polymer Networks and Reated Materialsvd. New York, 1981, p.^pp. Pages.
[17] J. R. Miller, J. Chem. Soc, p. 1311, 1960.
[18] J. W. Aylsworth, "US Pat.1," pp. 111-284, 1914.
[19] L. H. Sperling and D. W. Friedman, J. Polym. Sci.A, vol. 2, p. 425, 1969.
[20] H. L. Frisch, D. Klempner, and K. C. Frish, Polymer Eng & Sci, vol. 14, 1974.
[21] L. H. Sperling, R. R. Arnts, and J. Appl, Polym Sci, 1971.
[22] L. H. Sperling, "Macromol. Rev," J. Polym. Sci, vol. 12, pp. 141-180, 1977.
[23] L. H. Sperling, Polym. Eng. Sci., pp. 10-327, 1970.
[24] D. A. Thimas and L. H. Spering, Polymer Blends, vol. 1, 1976.
[25] L. H. Sperling, Ed., Multicomponent Polymer Material (American Chemical. Washington, 1986, p.^pp. Pages.
[26] C. K. Riew, Ed., Rubber-Toughened Plastics. Wastington: American Chemical Society, 1989, p.^pp. Pages.
[27] D. G. Shin, S. M. Shin, Y. C. Kim, H. Sun, and H. Myung, "Morphology anad Mechanical Properties of Siloxane-Modified Epoxy Systems."
[28] S. M. Shin, D. J. Byun, B. G. Min, Y. C. Kim, and D. K. Shin, Eds., Study of Siloxane-Modified Epoxy Resin Using Thermally Stimulated Current. 1995, p.^pp. Pages.
[29] J. I. Meijerink, S. Eguchi, M. Ogata, T. Ishii, S. Amagi, S. Numata, et al., Eds., The influence of Siloxane Modifiers on the Thermal Expansion Coefficient of Epoxy Resins. Polymer, 1994, p.^pp. Pages.
[30] M. Ochi, T. Katayama, K. Mimura, and H. Yamana, Eds., Effects of the Addition of Silicone Block Copolymers on the Toughness of Cured Epoxy Resin Modifed RTV-Silicone. J. Polym. Sci and Technol, 1993, p.^pp. Pages.
[31] T. H. HO and C. S. Wang, "Low-Stress Encapsulants by Vunylsiloxane Modification," Polym. Sci, pp. 51-2047, 1994.
[32] N. Terae, Y. Iguchi, and M. Sudo, Eds., Ultrafine Epoxy Silicone Rubber Powder. p.^pp. Pages.
[33] US Patent, 1992.
[34] S. Imai and O. Aoki, 1992.
[35] S. Zheng, H. Wang, Q. Dai, X. Kuo, D. Ma, and K. Wang, "Morphology and Structure of Organosilicon Polymer-Modified Epoxy Resin," Macromol. Chem. Phys, pp. 196-269, 1995.
[36] A. Apicella, "Effect of chemorheology on epoxy resin properties," in Developments in Reinforced Plastics—5, ed: Springer, 1986, pp. 151-180.
[37] H. Aguiar, J. Serra, P. Gonzalez, and B. Leon, "Structural study of sol–gel silicate glasses by IR and Raman spectroscopies," Journal of Non-Crystalline Solids, vol. 355, pp. 475-480, 2009.
[38] R. Almeida, T. Guiton, and C. Pantano, "Characterization of silica gels by infrared reflection spectroscopy," Journal of Non-Crystalline Solids, vol. 121, pp. 193-197, 1990.
[39] M. Nakamura, Y. Mochizuki, K. Usami, Y. Itoh, and T. Nozaki, "Infrared absorption spectra and compositions of evaporated silicon oxides (SiO< sub> x</sub>)," Solid State Communications, vol. 50, pp. 1079-1081, 1984.
[40] A. Burneau and C. Carteret, "Near infrared and ab initio study of the vibrational modes of isolated silanol on silica," Physical Chemistry Chemical Physics, vol. 2, pp. 3217-3226, 2000.
[41] D. Rajput, L. Costa, A. Terekhov, K. Lansford, and W. Hofmeister, "Silica coating of polymer nanowires produced via nanoimprint lithography from femtosecond laser machined templates," Nanotechnology, vol. 23, p. 105304, 2012.
[42] J. Lee, F. Jin, S. Park, and J. Park, "Study of new fluorine-containing epoxy resin for low dielectric constant," Surface and Coatings Technology, vol. 180, pp. 650-654, 2004.
[43 ]http://www.chemistry.ccsu.edu/glagovich/teaching/316/ir/amine.html
[44] http://orgchem.colorado.edu/Spectroscopy/irtutor/aminesir.html